A method for adjusting gas parameters of a reaction kettle

Abstract

The application discloses a gas parameter adjusting method for a reaction kettle and belongs to the field of high-temperature and high-pressure equipment control. The gas parameter adjusting method for the reaction kettle adjusts and controls the gas temperature and pressure in the control kettle and the reaction kettle through adjusting the gas booster and the heating belt, realizes two-stage accurate regulation and control of the gas temperature, pressure, concentration and other parameters before and after entering the kettle and real-time dynamic supplement, guarantees high consistency between the test working condition in the kettle and the field working condition; on the other hand, the application solves the problem that the gas composition and the proportioning accuracy in the reaction kettle are reduced due to the fact that the mixed gas formed by the reaction medium solution volatilization and the reaction gas under the simulated actual working condition cannot be realized in real time and accurately during the reaction gas proportioning process, thereby guaranteeing the high consistency between the test environment in the reaction kettle and the actual working condition and the reliability of the test result, and significantly improving the safety.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of high-temperature and high-pressure equipment control, in particular to a gas parameter adjusting method for a reaction kettle. BACKGROUND

[0002] The reaction kettle is one of the main equipment for the laboratory to carry out material corrosion performance evaluation. In the field of corrosion resistance evaluation of oil and gas field materials, the reaction kettle is generally used to carry out indoor simulation of the corrosion behavior of materials under the working conditions of oil and gas fields. The existing reaction kettle generally charges hydrogen sulfide, carbon dioxide, oxygen, nitrogen and other gases into the reaction kettle through a booster pump to reach the set pressure value, and then heats up to the test temperature and starts the test. However, during the process of gas entering the reaction kettle, the flow and pressure of different gases cannot be accurately measured during the process of entering, and the accurate proportioning of different gases in the reaction kettle cannot be achieved. Secondly, under actual high-temperature working conditions, the reaction solution medium volatilizes due to high temperature, resulting in actual reaction gas containing "mixed gas" formed by volatilization of the reaction medium solution. With the progress of the reaction in the kettle, the actual pressure decreases as the "mixed gas" is gradually consumed, but it cannot be supplemented in time. More importantly, it is impossible to accurately monitor and achieve real-time and accurate proportioning of "mixed gas", so as to accurately simulate the actual working conditions, resulting in a large deviation between the corrosion rate measured in the laboratory and the actual working conditions in the oil and gas field. Finally, a few improved devices (such as patents CN 109529723B and CN 11729612B) can enhance the monitoring of the concentration of the gas entering the reaction kettle to a certain extent by adding concentration probes and buffer tanks beside the reaction kettle, but they can only supplement the total amount of mixed gas by pressure, and still cannot accurately adjust the single gas source according to the actual gas type. More importantly, it is impossible to supplement the "mixed gas" formed by the volatilization of the reaction solution and the reaction gas in real time and accurately under actual working conditions, so as to obtain the corrosion test results based on the actual working conditions. SUMMARY

[0003] The purpose of the present application is to overcome the shortcomings of the prior art and provide a gas parameter adjusting method for a reaction kettle.

[0004] To achieve the above purpose, the present application adopts the following technical solutions:

[0005] A gas parameter adjusting method for a reaction kettle is based on a gas parameter adjusting system for a reaction kettle, which comprises the following steps:

[0006] Step 1: charge the reaction medium solution into the reaction kettle and the control kettle;

[0007] The various gases in the reaction gas source are respectively collected at the first check valve according to the test set proportion through the first pressure reducing valve connected thereto, heated through the first temperature control heating belt and pressurized through the gas booster after passing through the first check valve, and then sequentially enter the control kettle and the reaction kettle. The second temperature sensor and the first pressure sensor on the control kettle collect the temperature and pressure of the gas in real time, and the gas concentration probe in the control kettle collects the concentration value of various gases in the control kettle in real time. The collected temperature, pressure and concentration are compared with the corresponding test set value. The third temperature sensor and the second pressure sensor on the reaction kettle collect the temperature and pressure of the gas in real time, and the gas concentration probe in the reaction kettle collects the concentration value of various gases in the reaction kettle in real time. The collected temperature, pressure and concentration are compared with the corresponding test set value. According to the comparison result, the parameters of any one or more of the reaction gas source, the first temperature control heating belt, the gas booster, the second temperature control heating belt and the third temperature control heating belt are adjusted until the concentration, pressure and temperature of the gas in the control kettle and the reaction kettle reach the test set value, realizing primary regulation and correction.

[0008] Step two, as the test is carried out in the reaction kettle, when the data collected by the second gas concentration probe or the second pressure sensor drops to the preset value, the fifth check valve is opened to make the gas in the control kettle enter the reaction kettle until the concentration and pressure of the gas in the reaction kettle recover to the test set value.

[0009] Step three, the same gas as the test working condition parameters is supplemented into the control kettle through the first temperature control heating belt and the gas booster, and according to the change of the liquid level meter, the second check valve and the third check valve are opened. The reaction medium solution in the reaction medium storage enters the control kettle to supplement the reaction medium solution in the control kettle, so that the gas phase temperature and pressure and the liquid level in the control kettle are finally restored to the reaction set parameter value, realizing secondary regulation and correction.

[0010] Step four, steps two and three are continuously cycled until the test is completed.

[0011] The gas parameter adjusting system for the reaction kettle comprises a reaction gas source, a first pressure reducing valve is arranged on a connecting pipeline of each gas source tank in the reaction gas source, the outlets of the first pressure reducing valves are gathered in one pipeline through a pipeline, a first temperature control heating belt and a gas booster are arranged on the pipeline in sequence, the pipeline at the outlet of the gas booster is divided into two routes, one route is connected with the inlet of a reaction medium storage through a second one-way valve, the outlet of the reaction medium storage is connected with the liquid inlet of a control kettle through a third one-way valve, the other route is connected with the gas inlet of the control kettle through a fourth one-way valve, the outlet of the control kettle is connected with the inlet of the reaction kettle through a fifth one-way valve, and the outlet of the reaction kettle is used for discharging reaction exhaust gas; a liquid level meter, a second temperature control heating belt, the fourth one-way valve, a second temperature sensor, a first pressure sensor and a first gas concentration probe are arranged on the control kettle; a third temperature control heating belt, a gas concentration probe, a third temperature sensor and a second pressure sensor are arranged on the reaction kettle; reaction medium solutions are arranged in the reaction medium storage, the control kettle and the reaction kettle; and the reaction gas source, the first temperature control heating belt, the gas booster, the second temperature control heating belt and the third temperature control heating belt are controlled by PCL.

[0012] Further, the volume of the reaction medium solution in the reaction kettle and the control kettle in step one is the same.

[0013] Further, the volume and structure of the control kettle and the reaction kettle of the gas parameter adjusting system for the reaction kettle are the same.

[0014] Further, when the pressure collected by the first pressure sensor is greater than a safety threshold, the gas is discharged by the first safety valve, until the pressure collected by the first pressure sensor is below the safety threshold.

[0015] Further, the outlet of the reaction kettle in the gas parameter adjusting system for the reaction kettle is connected with an exhaust gas treatment device.

[0016] Further, in step two, the tail gas of the reaction kettle after the test is completed is discharged into the exhaust gas collection and treatment device through the second pressure reducing valve and the sixth one-way valve.

[0017] Further, when the pressure of the reaction kettle collected by the second pressure sensor is greater than a safety threshold, the gas in the reaction kettle is discharged by the second safety valve, until the pressure collected by the second pressure sensor is below the safety threshold.

[0018] Further, a first temperature sensor is arranged on the pipeline at the outlet of the gas booster in the gas parameter adjusting system for the reaction kettle.

[0019] When the adjustment is carried out, the temperature collected by the first temperature sensor is compared with the set temperature, until the set temperature is reached, the fourth one-way valve is opened, and the gas at the outlet of the gas booster enters the regulation kettle.

[0020] Further, the reaction medium solution is a NaCl type solution.

[0021] Compared with the prior art, the present application has the following beneficial effects:

[0022] The gas parameter adjustment method for the reaction kettle of the present application realizes the control of the gas temperature and pressure in the regulation kettle and the reaction kettle through the adjustment of the gas booster and the heating belt, realizes the secondary precise adjustment and real-time dynamic supplement of the gas temperature, pressure, concentration and other parameters before and after entering the kettle, guarantees the high consistency of the test working condition in the kettle and the field working condition; on the other hand, the present application solves the problem that the gas composition and ratio precision in the reaction kettle is reduced due to the inability to realize the "mixed gas" formed by the reaction medium solution volatilization and the reaction gas under the simulated actual working condition in real time and accurately during the reaction gas ratio process, thereby guaranteeing the high consistency of the test environment in the reaction kettle and the actual working condition and the reliability of the test results, and significantly improving the safety.

[0023] Further, through the linkage of the gas booster, the regulation kettle, the reaction kettle, the pressure sensor, the temperature sensor, the safety valve and other devices connected respectively, timely pressure relief is realized, and the high safety of the whole system operation is realized.

[0024] Further, when the reaction medium solution is a NaCl type solution, the NaCl type solution generally contains CO3 2- , HCO3 - , S 2- , H + , etc., the HCO3 - in the NaCl type solution will decompose to generate CO2 gas above 50℃, and H + is easy to react with HCO3 - , S 2- to generate H2S and CO2 gas under heating. BRIEF DESCRIPTION OF DRAWINGS

[0025] Figure 1 It is a structural schematic diagram of the system of the present application.

[0026] Wherein, 1-reaction gas source; 2-first pressure reducing valve; 3-first check valve; 4-first temperature control heating belt; 5-gas booster; 6-first temperature sensor; 7-second check valve; 8-first reaction medium solution; 9-reaction medium storage; 10-third check valve; 11-second reaction medium solution; 12-regulating kettle; 13-liquid level meter; 14-second temperature control heating belt; 15-fourth check valve; 16-second temperature sensor; 17-first pressure sensor; 18-first safety valve; 19-first gas concentration probe; 20-third temperature control heating belt; 21-reaction kettle; 22-third reaction medium solution; 23-second gas concentration probe; 24-fifth check valve; 25-third temperature sensor; 26-second pressure sensor; 27-second safety valve; 28-second pressure reducing valve; 29-sixth check valve; 30-waste gas collection and treatment device. DETAILED DESCRIPTION

[0027] For those skilled in the technical field, the technical solutions in the embodiments of the present application will be described clearly and completely below in conjunction with the accompanying drawings in the embodiments of the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor should belong to the scope of protection of the present application.

[0028] It should be noted that the terms "first", "second" and the like in the specification and claims of the present application and the above-described drawings are used to distinguish similar objects, and do not necessarily have to describe a specific order or sequence. It should be understood that the data thus used can be interchanged under appropriate circumstances, so that the embodiments of the present application described herein can be implemented in an order other than that illustrated or described herein. In addition, the terms "include" and "have" and any variations thereof are intended to cover non-exclusive inclusion, for example, a process, method, system, product or device including a series of steps or units does not have to be limited to only those steps or units clearly listed, but can include other steps or units not clearly listed or inherent to these processes, methods, products or devices.

[0029] In view of the above problems, it is urgent to develop a reaction kettle reaction gas precise regulation system which can accurately control the reaction gas and has high safety, so as to overcome the shortcomings of the existing reaction kettle reaction gas stratification under high temperature, unable to accurately adjust the ratio of multiple gases in real time, and the safety hidden danger caused by the additional booster device, significantly improve the corrosion gas concentration precise regulation in the reaction kettle and the safety of the whole system, so as to realize the maximum reduction of oil and gas field working conditions.

[0030] The present application will be described in further detail below in conjunction with the accompanying drawings:

[0031] Referring to Figure 1 , Figure 1 It is the system structure schematic diagram of the present application; a gas parameter adjusting system for reaction kettle, comprising reaction gas source 1, first pressure reducing valve 2 is respectively arranged on the connecting pipeline of each gas source tank in reaction gas source 1, the outlet of first pressure reducing valve 2 is gathered in a pipeline through pipeline, the pipeline is provided with first temperature control heating band 4 and gas booster 5 in turn;

[0032] The pipeline at the outlet of gas booster 5 is divided into two ways, one way is connected with the inlet of reaction medium storage 9 through second one-way valve 7, the outlet of reaction medium storage 9 is connected with the liquid inlet of control kettle 12 through third one-way valve 10, the other way is connected with the gas inlet of control kettle 12 through fourth one-way valve 15; the outlet of control kettle 12 is connected with the inlet of reaction kettle 21 through fifth one-way valve 24, and the outlet of reaction kettle 21 is used to discharge reaction exhaust gas;

[0033] Second temperature control heating band 14, fourth one-way valve 15, second temperature sensor 16, first pressure sensor 17 and first gas concentration probe 19 are arranged on the control kettle 12;

[0034] Third temperature control heating band 20, gas concentration probe 23, third temperature sensor 25 and second pressure sensor 26 are arranged on the reaction kettle 21;

[0035] Reaction medium storage 9, control kettle 12 and reaction kettle 21 are all filled with reaction medium solution;

[0036] Reaction gas source 1, first temperature control heating band 4, gas booster 5, second temperature control heating band 14 and third temperature control heating band 20 are all controlled by PCL;

[0037] The adjusting process of the present application is as follows:

[0038] Reaction medium solution is filled in reaction kettle 21 and control kettle 12;

[0039] The various gases in the reaction gas source 1 are respectively collected at the first check valve 3 through the first pressure reducing valve 2 connected thereto according to the test set ratio, heated and pressurized by the first temperature control heating belt 4 and the gas booster 5 after passing through the first check valve 3, and then sequentially enter the control kettle 12 and the reaction kettle 21. The second temperature sensor 16 and the first pressure sensor 17 on the control kettle 12 collect the temperature and pressure of the gas in real time, the gas concentration probe 19 in the control kettle 12 collects the concentration value of various gases in the control kettle 12 in real time, and the collected temperature, pressure and concentration are compared with the corresponding test set value. The third temperature sensor 25 and the second pressure sensor 26 on the reaction kettle 21 collect the temperature and pressure of the gas in real time, and the gas concentration probe 23 in the reaction kettle 21 collects the concentration value of various gases in the reaction kettle 21 in real time. The collected temperature, pressure and concentration are compared with the corresponding test set value, and the parameters of any one or more of the reaction gas source 1, the first temperature control heating belt 4, the gas booster 5, the second temperature control heating belt 14 and the third temperature control heating belt 20 are adjusted according to the comparison result, until the concentration, pressure and temperature of the gas in the control kettle 12 and the reaction kettle 21 reach the test set value, realizing primary regulation and correction.

[0040] With the test in the reaction kettle 21, when the data collected by the second gas concentration probe 23 or the second pressure sensor 26 drops to the preset value, the fifth check valve 24 is opened to make the gas in the control kettle 12 enter the reaction kettle 21, until the concentration and pressure of the gas in the reaction kettle 21 recover to the test set value. Then, the same gas as the test working condition parameters is supplemented into the control kettle 12 through the first temperature control heating belt 4 and the gas booster 5, and according to the change of the liquid level meter 13, the second check valve 7 and the third check valve 10 are opened, the reaction medium solution in the reaction medium reservoir 9 enters the control kettle 12 to supplement the reaction medium solution in the control kettle 12, finally ensuring that the gas phase temperature and pressure and the liquid level in the control kettle 12 recover to the reaction set parameter value, realizing secondary regulation and correction.

[0041] The first safety valve 18, the second safety valve 27 are respectively linked with the first pressure sensor 17, the second pressure sensor 26 and the first temperature sensor 6, the second temperature sensor 16, the third temperature sensor 25, when the pressure of the gas pipeline and the control kettle 12 and the reaction kettle 21 exceeds the set value, the safety valve responds in real time and immediately releases pressure to the safety pressure range, and adjusts the first temperature control heating belt 4, the second temperature control heating belt 14 and the third temperature control heating belt 20 to the set temperature, thereby significantly improving the safety performance of the whole system.

[0042] With the reaction, the reaction exhaust gas in the reaction kettle 21 is collected and treated by the waste gas collection and treatment device 30 in real time.

[0043] The adjusting principle of the present application is:

[0044] First, the reaction medium solution is respectively filled into the reaction medium storage 9, the control kettle 12 and the reaction kettle 21, the volume of the reaction medium in the control kettle 12 and the reaction kettle 21 is the same; through the parameters collected by the temperature sensor and the pressure sensor on the control kettle 12 and the reaction kettle 21, the control reaction gas source 1, the first temperature control heating belt 4 and the gas booster 5 make the gas phase temperature and pressure and the liquid phase volume in the control kettle 12 and the reaction kettle 21 reach the test set parameters, realizing the first order adjustment and correction.

[0045] With the test in the reaction kettle 21, the mixed gas in the reaction kettle 21 is gradually consumed due to the reaction with the sample, resulting in the decrease of the gas pressure and the liquid phase content in the reaction kettle 21, and then the difference between the corrosion environment and the actual working condition. The present application sets the control kettle 12 which is completely the same as the reaction kettle 21, including the kettle volume, the gas pressure and temperature in the kettle and the auxiliary detection instruments such as the liquid level meter, the gas concentration probe, etc. When the gas and the liquid phase in the reaction kettle are consumed, the reaction gas which is completely the same as the actual working condition is fed into the reaction kettle through the control kettle in real time, so as to ensure that the corrosion environment in the reaction kettle is the same as the oilfield actual working condition environment at all times; secondly, the gas which is the same as the test working condition parameters is supplemented into the control kettle 12 through the first temperature control heating belt 4 and the gas booster 5, and according to the change of the liquid level meter 13, the first reaction medium solution 8 is supplemented into the control kettle 12 through the reaction medium storage 9, finally ensuring that the gas phase temperature and pressure and the liquid phase height in the control kettle 12 are restored to the reaction set parameter value, realizing the second order adjustment and correction.

[0046] Under the actual working condition of the oilfield, the real environment of the pipe corrosion reaction is mainly composed of the "mixed gas" formed by the high temperature and high pressure corrosion gas and the liquid phase volatilization at high temperature, especially the strong corrosive CO2 and H2S gas. Therefore, when the corrosion simulation test is carried out in the laboratory, the "mixed gas" composed of the gas phase and the liquid phase volatilization is continuously consumed in the reaction kettle with the reaction. Therefore, in order to realize the accurate simulation of the actual working condition of the oil and gas field, the "mixed gas" formed by the corrosion gas and the reaction liquid phase medium volatilization must be supplemented in real time, so as to meet the real requirements of the oil and gas field actual working condition environment, so as to obtain the highly accurate simulation test condition.

[0047] The preferred embodiments of the present application will be described in detail below with reference to the accompanying Figure 1 The preferred embodiments of the present application will be described in detail below with reference to the accompanying

[0048] Example 1

[0049] According to the test conditions, the reaction gas is set as single gas CO2, the reaction medium solution is set as NaCl type solution, the reaction gas pressure is set as 5 MPa and the temperature is set as 100℃, the first reaction medium solution is set as 5L, and the second reaction medium solution and the third reaction medium solution are both set as 3L.

[0050] According to the test conditions, the parameters of each functional unit of the high-temperature and high-pressure reaction kettle reaction gas precision adjusting system are set. Specifically, the pressure and temperature values of the first temperature control heating belt 4, the gas booster 5, the second temperature control heating belt 14, and the third temperature control heating belt 20 are set for testing, and the first temperature sensor 6, the second temperature sensor 16, the third temperature sensor 25, the first pressure sensor 17, and the second pressure sensor 26 are used for real-time monitoring of the pressure and temperature values. The volume of the first reaction medium solution is set as 5L, the volume of the second reaction medium solution and the third reaction medium solution are both set as 3L, and the liquid level meter 13 is used for detecting the volume of the second reaction medium solution 11.

[0051] Further, the gas source CO2 is sequentially passed through the first pressure reducing valve 2, the first check valve 3, the first temperature control heating belt 4, and the gas booster 5 to be heated and pressurized to 5 MPa and 90℃, and parameter measurement is performed. Figure 1 As shown in FIG. 1, the second temperature sensor 16 and the first pressure sensor 17 are used to monitor the temperature and pressure of CO2 in the control kettle 12; the third temperature sensor 25 and the second pressure sensor 26 are used to monitor the temperature and pressure of CO2 in the reaction kettle 21; the temperature and pressure detection data of the control kettle 12 and the reaction kettle 21 are fed back to the gas booster 5 and the first temperature control heating belt 4 in real time, and the output CO2 pressure and temperature are adjusted and corrected to 5 MPa and 90℃.

[0052] Specifically, the first temperature sensor 6, the second temperature sensor 16, the first pressure sensor 17, the gas booster 5, and the first temperature control heating belt 4 are set in linkage program integrated in the PLC central control console.

[0053] Specifically, the second gas concentration probe 23, the third temperature sensor 25, the second pressure sensor 26, the first gas concentration probe 13, the second temperature control heating belt 14, the second temperature sensor 16, and the first pressure sensor 17 are used to measure the temperature and pressure of high-temperature and high-pressure CO2, and are fed back to the reaction gas source 1, the gas booster 5, and the first temperature control heating belt 4 in real time, so that the temperature and pressure of the gas in the control kettle 12 and the reaction kettle 21 are adjusted and corrected to 5 MPa and 90℃.

[0054] Further, the reaction medium storage 9 contains 5L of reaction medium solution 8,

[0055] Further, the regulating kettle 12 is filled with 3L of reaction medium solution 11.

[0056] Specifically, the liquid level meter 13 monitors the volume change of the reaction medium solution 11 by liquid level scale change.

[0057] Specifically, when the volume of the reaction medium solution 22 is less than 3L, no reaction medium solution is added to the reaction kettle 22.

[0058] Further, the temperature control heating belt on the gas conveying pipeline between the regulating kettle 12 and the reaction kettle 21 is set to a heating temperature of 90℃.

[0059] Further, as the reaction proceeds, the gas pressure and temperature in the reaction kettle 21 are lower than 5MPa and 90℃, and the volume of the reaction medium solution 22 is less than 3L. The third temperature sensor 25, the second pressure sensor 26, and the second temperature sensor 16, the first temperature sensor 6, and the first pressure sensor 17 are linked and real-time feedback to the gas booster 5 and the first temperature control heating belt 4, the second temperature control heating belt 14, and the reaction gas source 1 through PLC central control to adjust and correct the gas pressure, temperature, and concentration in the reaction kettle 21 to 5MPa and 90℃. The specific operation method is: when the third temperature sensor 26, the second pressure sensor 17, and the third gas concentration probe 23 detect that the temperature, pressure, and various gas concentrations in the reaction kettle 21 decrease, immediately supplement into the reaction kettle 21 through the one-way valve 24 of the regulating kettle 12 to ensure that the CO2 pressure and temperature in the reaction kettle 21 are accurately adjusted to 5MPa and 90℃; and then the CO2 pressure and temperature in the regulating kettle 12 are accurately adjusted to 5MPa and 90℃ through the reaction source 1, the first temperature control heating belt 4, the gas booster 5, the first temperature sensor 4, the second temperature control heating belt 14, the second temperature sensor 16, and the first pressure sensor 17.

[0060] Further, the reaction kettle 21 is filled with 3L of reaction medium solution 22.

[0061] Specifically, when the volume of the reaction medium solution 22 is less than 3L, no reaction medium solution is added to the reaction kettle 22.

[0062] Further, the first safety valve 18, the second safety valve 27, and the first temperature sensor 6, the second temperature sensor 16, and the third temperature sensor 26 are linked and real-time monitoring and adjustment of gas pressure, concentration, temperature, and other parameters are carried out through PLC central control.

[0063] Specifically, when the CO2 pressure and temperature in the gas pipeline and the conditioning kettle 12 and the reaction kettle 21 exceed 5 MPa and 90°C, the safety valve responds in real time and immediately releases pressure to equal 5 MPa, while adjusting the first temperature control heating band 4, the second temperature control heating band 14, and the third temperature control heating band 20 to 90°C.

[0064] Further, the reaction exhaust gas in the reaction kettle 21 enters the exhaust gas collection and treatment device 30 for harmless environmental protection treatment through the second pressure reducing valve 28 and the sixth one-way valve 29.

[0065] Example 2

[0066] The test working conditions are set as various corrosive gases such as H2S, CO2, SiO2, CH4, and O2, and the reaction total gas pressure value is 15 MPa and the temperature is 120°C, the concentration ratio of each corrosive gas is H2S:CO2:SiO2:CH4:O2 = 1:2:1:1:2, the first reaction medium solution 8 is 10 L, and the second reaction medium solution 11 and the second reaction medium solution 22 have the same volume, both of which are 5 L. This is an example, but it is not limited thereto. The system described in the present application can realize precise adjustment of the temperature, pressure, and concentration of any gas at any ratio and ensure the safety of system operation. According to the set test working condition, the parameters of each functional unit of the high-temperature and high-pressure reaction kettle reaction gas precise adjustment system are set in sequence.

[0067] Specifically, the temperature and pressure values of the first temperature control heating band 4, the gas booster 5, the second temperature control heating band 14, the third temperature control heating band 20, and other devices are set to be the same as the test working conditions; at the same time, the first temperature sensor 6, the second temperature sensor 16, the third temperature sensor 25, the first pressure sensor 17, and the second pressure sensor 26 are used for real-time monitoring of the pressure and temperature values. That is, the reaction total gas pressure value is 15 MPa and the temperature is 120°C, the concentration ratio of each gas is H2S:CO2:SiO2:CH4:O2 = 1:2:1:1:2, the volume of the first reaction medium solution is set to be 10 L, and the second and third reaction medium solutions are both 5 L, and the liquid level meter 13 is used to monitor the volume of the second reaction medium solution 11.

[0068] In combination Figure 1H2S, CO2, SiO2, CH4and O2in the reaction gas source 1 are collected at the first one-way valve 3 through the first pressure reducing valve 2 according to the test set ratio H2S:CO2:SiO2:CH4:O2=1:2:1:1:2, and then are heated by the first temperature control heating belt 4 and pressurized by the gas booster 5 in sequence before being input into the control kettle 12 and the reaction kettle 21. The first temperature sensor 6, the second temperature sensor 16, the first pressure sensor 17 and the first gas concentration probe 19 collect and output the temperature, pressure and concentration of various gases in the control kettle 12 in real time; the third temperature sensor 25 and the second pressure sensor 26 are used to monitor the temperature and pressure of various gases in the reaction kettle; the measured temperature and pressure detection data of the control kettle 12 and the reaction kettle 21 are fed back to the gas booster 5 and the first temperature control heating belt 4 in real time online. When the concentration of a certain gas component does not reach the test set concentration, the temperature and partial pressure are adjusted by the reaction source 1, the first temperature control heating belt 4, the gas booster 5, the first temperature sensor 6, the second temperature sensor 16, the first pressure sensor 17, the second temperature control heating belt 14, the first concentration probe 19 and the like until the output gas reaches the test set 15 MPa, 120℃ and H2S:CO2:SiO2:CH4:O2=1:2:1:1:2, realizing the first order regulation and correction.

[0069] Further, as the reaction proceeds, the pressure and temperature of the various gases in the reactor 21 are lower than 15 MPa and 120°C due to reaction consumption, the concentration ratio of the various gases is H2S:CO2:SiO2:CH4:O2≠1:2:1:1:2, and the volume of the reaction medium solution 22 is less than 5 L due to reaction consumption. By linking the third temperature sensor 25, the second gas concentration probe 23, the second pressure sensor 26, and the second temperature sensor 16, the first temperature sensor 6, and the first pressure sensor 17, and by PLC central control, real-time feedback is provided to the gas booster 5 and the first temperature-controlled heating belt 4, the second temperature-controlled heating belt 14, and the reaction gas source 1 to perform secondary regulation and correction of the pressure, temperature, and concentration of the various gases in the reactor 21 to 15 MPa and 120°C, and the concentration ratio of the various gases is H2S:CO2:SiO2:CH4:O2=1:2:1:1:2. The specific operation method is as follows: when the third temperature sensor 26, the second pressure sensor 17, and the third gas concentration probe 23 detect that the temperature, pressure, and concentration ratio of the various gases in the reactor 21 decrease or decrease, the reaction medium solution 22 is immediately supplemented into the reactor 21 through the one-way valve 24 of the control tank 12, and the second pressure sensor 26 and the third temperature sensor 25 are used to ensure that the CO2 pressure and temperature in the reactor 21 are regulated to 15 MPa and 120°C, and the concentration ratio of the various gases is H2S:CO2:SiO2:CH4:O2=1:2:1:1:2. The CO2 pressure and temperature in the control tank 12 are monitored and regulated by the reaction source 1, the first temperature-controlled heating belt 4, the gas booster 5, the second temperature-controlled heating belt 14, the second temperature sensor 16, the first pressure sensor 17, and the first gas concentration probe 19, and the concentration ratio of the various gases is H2S:CO2:SiO2:CH4:O2=1:2:1:1:2.

[0070] Further, the reactor 21 is filled with 5 L of reaction medium solution 22.

[0071] Specifically, when the volume of the reaction medium solution 22 is less than 5 L, the reaction medium solution is not supplemented into the reactor 22.

[0072] Further, the first safety valve 18 and the second safety valve 27 are linked to the first pressure sensor 17, the second pressure sensor 26, the first temperature sensor 6, the second temperature sensor 16, and the third temperature sensor 26, respectively, and real-time monitoring and regulation of the gas pressure, concentration, and temperature parameters are performed by PLC central control.

[0073] Specifically, when the CO2 pressure and temperature in the gas pipeline and the control tank 12 and the reactor 21 exceed 15 MPa and 120°C, the safety valve responds immediately and releases pressure to 15 MPa, and the first temperature-controlled heating belt 4, the second temperature-controlled heating belt 14, and the third temperature-controlled heating belt 20 are adjusted to 120°C.

[0074] Further, the reaction exhaust gas in the reaction kettle 21 enters the exhaust gas collection and treatment device 30 through the second pressure reducing valve 28 and the sixth one-way valve 29 for harmless environmental protection treatment.

[0075] The gas parameter adjusting method for the reaction kettle is based on the gas parameter adjusting system for the reaction kettle, the system is provided with the control kettle and the reaction kettle in communication, the monitoring devices such as the pressure sensor, the temperature sensor and the gas concentration probe between the control kettle and the reaction kettle are linked with the control period such as the temperature control and heat tracing belt and the gas booster, the two-stage control and correction and the real-time dynamic supplement of the gas temperature, pressure, concentration and other parameters before and after entering the kettle can be realized; at the same time, the reaction medium storage, the liquid level meter and other devices and the real-time supplement of the reaction medium solution are set, the "mixed gas" composed of the reaction gas and the medium solution high-temperature volatile gas is obtained, so that the high consistency of the test working condition in the reaction kettle and the real working condition of the oil and gas field is ensured; in addition, the gas booster, the control kettle and the reaction kettle are respectively connected with the pressure sensor, the temperature sensor, the safety valve and other devices, the high safety of the whole system operation is realized. The present application not only can realize the real-time dynamic accurate control of the reaction gas in the reaction kettle, but also solves the problem that the existing high-temperature and high-pressure kettle cannot restore the real corrosion working condition of the oil field in real time and accurately, so as to ensure the high consistency of the test environment in the reaction kettle and the real working condition of the oil and gas field and the reliability of the test result, and significantly improve the safety of the adjusting process.

[0076] The above content only illustrates the technical idea of the present application, and cannot limit the protection scope of the present application, any modification made according to the technical idea of the present application on the basis of the technical scheme falls within the protection scope of the present application.

Claims

1. A method for adjusting a gas parameter of a reaction vessel, characterized by, Based on the gas parameter adjustment system for the reaction kettle, the method comprises the following steps: Step one, fill the reaction medium solution into the reaction kettle (21) and the control kettle (12); The control reaction gas source (1) is connected with the first pressure reducing valve (2), and the first pressure reducing valve (2) is connected with the first one-way valve (3). The first one-way valve (3) is connected with the first temperature control heating belt (4), and the first temperature control heating belt (4) is connected with the gas booster (5). The gas booster (5) is connected with the control kettle (12) and the reaction kettle (21) in sequence. The second temperature sensor (16) and the first pressure sensor (17) on the control kettle (12) collect the temperature and pressure of the gas in real time. The gas concentration probe (19) in the control kettle (12) collects the concentration value of various gases in the control kettle (12) in real time. The collected temperature, pressure and concentration are compared with the corresponding test set value. The third temperature sensor (25) and the second pressure sensor (26) on the reaction kettle (21) collect the temperature and pressure of the gas in real time. The gas concentration probe (23) in the reaction kettle (21) collects the concentration value of various gases in the reaction kettle (21) in real time. The collected temperature, pressure and concentration are compared with the corresponding test set value. According to the comparison result, the parameters of any one or more of the reaction gas source (1), the first temperature control heating belt (4), the gas booster (5), the second temperature control heating belt (14) and the third temperature control heating belt (20) are adjusted, until the concentration, pressure and temperature of the gas in the control kettle (12) and the reaction kettle (21) reach the test set value, realizing primary regulation and correction; Step two, as the test in the reaction kettle (21) is carried out, when the data collected by the second gas concentration probe (23) or the second pressure sensor (26) drops to the preset value, the fifth one-way valve (24) is opened to make the gas in the control kettle (12) enter the reaction kettle (21), until the concentration and pressure of the gas in the reaction kettle (21) recover to the test set value; Step three, the first temperature control heating belt (4) and the gas booster (5) are used to supplement the gas with the same test working condition parameters into the control kettle (12). According to the change of the liquid level meter (13), the second one-way valve (7) and the third one-way valve (10) are opened, the reaction medium solution in the reaction medium storage (9) enters the control kettle (12), the reaction medium solution in the control kettle (12) is supplemented, and finally the gas phase temperature and pressure and the liquid level in the control kettle (12) recover to the reaction set parameter value, realizing secondary regulation and correction; Step four, continuously circulate step two and step three until the test is completed. The gas parameter adjusting system for the reaction kettle comprises a reaction gas source (1), a first pressure reducing valve (2) is arranged on the connecting pipeline of each gas source tank in the reaction gas source (1), the outlet of the first pressure reducing valve (2) is gathered in a pipeline, a first temperature control heating belt (4) and a gas booster (5) are arranged on the pipeline in sequence, the pipeline at the outlet of the gas booster (5) is divided into two routes, one route is connected with the inlet of a reaction medium storage (9) through a second one-way valve (7), the outlet of the reaction medium storage (9) is connected with the liquid inlet of a control kettle (12) through a third one-way valve (10), the other route is connected with the gas inlet of the control kettle (12) through a fourth one-way valve (15), the outlet of the control kettle (12) is connected with the inlet of a reaction kettle (21) through a fifth one-way valve (24), and the outlet of the reaction kettle (21) is used for discharging reaction waste gas; a liquid level meter (13), a second temperature control heating belt (14), the fourth one-way valve (15), a second temperature sensor (16), a first pressure sensor (17) and a first gas concentration probe (19) are arranged on the control kettle (12); a third temperature control heating belt (20), a gas concentration probe (23), a third temperature sensor (25) and a second pressure sensor (26) are arranged on the reaction kettle (21); the reaction medium storage (9), the control kettle (12) and the reaction kettle (21) are all filled with reaction medium solution; and the reaction gas source (1), the first temperature control heating belt (4), the gas booster (5), the second temperature control heating belt (14) and the third temperature control heating belt (20) are all controlled by PCL.

2. The gas parameter adjustment method for a reaction vessel according to claim 1, wherein The volume of the reaction medium solution in the reaction kettle (21) and the control kettle (12) in step one is the same.

3. The gas parameter adjustment method for a reaction vessel according to claim 1, wherein The volume and structure of the control kettle (12) and the reaction kettle (21) of the gas parameter adjusting system for the reaction kettle are the same.

4. The gas parameter adjustment method for a reaction vessel according to claim 1, wherein When the pressure collected by the first pressure sensor (17) is greater than a safety threshold, the gas is discharged by the first safety valve (18) after the gas, and the pressure collected by the first pressure sensor (17) is below the safety threshold.

5. The gas parameter adjustment method for a reaction vessel according to claim 1, wherein The outlet of the reaction kettle (21) in the gas parameter adjusting system for the reaction kettle is connected with a waste gas treatment device (30).

6. The gas parameter adjustment method for a reaction vessel according to claim 5, wherein In step two, when the test is performed, the tail gas of the reaction kettle (21) after the test is discharged into the waste gas collection and treatment device (30) through the second pressure reducing valve (28) and the sixth one-way valve (29).

7. The gas parameter adjustment method for a reaction vessel according to claim 1, wherein When the pressure of the reaction kettle (21) collected by the second pressure sensor (26) is greater than a safety threshold, the gas in the reaction kettle (21) is discharged by the second safety valve (27) on the reaction kettle (21), and the pressure collected by the second pressure sensor (26) is below the safety threshold.

8. The gas parameter adjustment method for a reaction vessel according to claim 1, wherein A first temperature sensor (6) is arranged on the pipeline at the outlet of the gas booster (5) in the gas parameter adjusting system for the reaction kettle. When the adjustment is performed, the temperature collected by the first temperature sensor (6) is compared with the set temperature, the fourth one-way valve (15) is opened when the set temperature is reached, and the gas at the outlet of the gas booster (5) enters the control kettle (12).

9. The gas parameter adjustment method for a reaction vessel according to claim 1, wherein The reaction medium solution is a NaCl type solution. The reaction medium solution is a NaCl type solution.

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